Carbon Dioxide → 3-Methylthiotetrafluoropropionic acid

HRID 1632159

반응식

HRID 1632159 반응식
[CH3:1][SH:2].[H-].[Na+].[C:5](=[O:7])=[O:6].[F:8][C:9]([F:13])=[C:10]([F:12])[F:11].Cl>CS(C)=O.O>[CH3:1][S:2][C:10]([F:12])([F:11])[C:9]([F:13])([F:8])[C:5]([OH:7])=[O:6]

참가 물질

8

반응물 5

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 878MethanethiolHCID 8301TetrafluoroethyleneHCID 24758Sodium hydride

생성물 1

HCID 133288983-Methylthiotetrafluoropropionic acid수율 98.5%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

NaSCH3 was prepared by distilling 24 g (0.50 mol) of methyl mercaptan into a stirred suspension of 24 g (0.50 mol) of 50% NaH/mineral oil in 170 ml of dimethyl sulfoxide over a 2-hr period. The mixture was charged into a 400-ml tube with 27 g (0.6 mol) of CO2 and 50 g (0.50 mol) of tetrafluoroethylene and shaken at 50° for 8 hrs. The reaction mixture was poured into a cold solution of 300 ml of concentrated HCl in 1 liter of water, and the resulting mixture was extracted continuously with ether. Removal of volatiles from the extracts at 5 mm gave 94.6 g of 3-methylthiotetrafluoropropionic acid. This acid was stirred at 85° to 95° while a mixture of 125 ml (about 1.2 mol) of 30% H2O2 and 75 ml of acetic acid was added dropwise over 2 hrs. The mixture was stirred at 90° to 95° for 3 hrs more, then evacuated at full pump to remove volatiles.

후처리

  1. customNaSCH3 was prepared
  2. extractionthe resulting mixture was extracted continuously with ether
  3. customRemoval of volatiles from the extracts at 5 mm

출처 및 근거

ORD 기록
ord-b6b4b9bd9ef04e228107f97d7cccaa37
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04474700

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